Comparison between different fracture toughness techniques in zirconia dental ceramics.

Vickers indentation (IF) and single-edge-V-notched beam (SEVNB), to measure the fracture toughness (KIC ) of zirconia-based dental ceramics and mathematical models were proposed to establish a correlation between both. Zirconia (ZrO2 ) stabilized with 3 mol. % of Y2 O3 (3Y-TZP) and 5 mol% of Y2 O3 (5Y-PSZ) were compacted (n = 42) and sintered for 2 h at different temperatures (1475°C, 1500°C, 1550°C, or 1600°C). After sintering, they were characterized by relative density using the ASTM C373-88 standard, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The average grain size was measured according to the ASTM E1382-97 standard. The fracture toughness (KIC ) was determined using two methods: Vickers indentation fracture toughness (KIC-IF ): method based on mathematical modeling that considers the parameters used for the Vickers hardness test and Fracture toughness by the single-edge-V-notch-beam (KIC-SEVNB ): method proposed by ISO 23146:08. The main phases of the 3Y-TZP and 5Y-PSZ ceramics were ZrO2 -tetragonal and ZrO2 -cubic, respectively. The 3Y-TZP specimens showed equiaxed grains with average grain sizes ranging from 0.55 to 0.79 µm. The grain sizes of 5Y-PSZ of specimens sintered at 1475°C and 1600°C were 0.62 and 2.32 µm, respectively. For all ceramics the crack size ratio was c/a < 2.5, suggesting a Palmqvist-type crack system. The fracture toughness measured by the Vickers indentation method (KIC-IF ) and by the SEVNB method (KIC-SEVNB ) was the same when the experimental data were fit to a mathematical model.

Mechanical properties of ceramic composites based on ZrO2 co-stabilized by Y2O3-CeO2 reinforced with Al2O3 platelets for dental implants.

OBJECTIVES: The objective of this work was the development and characterization of a ceramic composite based on (Ce,Y)-TZP/Al2O3 aiming an application on dental implants, comparing it with conventional monolithic 3Y-TZP ceramics, currently used for the same type of application. METHODS: Ceramic samples, 3Y-TZP (n = 40) and (Ce,Y)-TZP/Al2O3 (n = 40), were sintered at 1500 °C - 2h and characterized by relative density, X-Ray diffraction (XRD) and microstructure. Then, the samples of both materials were divided into two groups: 1) samples with original (as sintered) surfaces; 2) samples with conditioned, polished, surfaces. All samples were submitted to hydrothermal degradation tests, on an autoclave (134 °C - 2 bar), for 10 h in artificial saliva. The degraded samples were characterized by XRD and the polished group were also characterized by their elastic moduli, Vickers hardness and fracture toughness (Vickers indentation method). Both groups were also submitted to a flexural strength test, 3B-P testing, for which the data were interpreted using Weibull statistics. RESULTS: All sintered specimens presented nearly full densification. After the hydrothermal degradation tests, 3Y-TZP samples presented 16.4% of monoclinic (m)-ZrO2 phase while the composite samples withheld 100% of tetragonal (t)-ZrO2 phase. Both materials presented equiaxial ZrO2 grains with an average size of 0.48 ± 0.17 µm and 0.75 ± 0.22 µm, respectively, for the monolithic and composite ceramics. In the composites, is observed the presence of well distributed Al2O3 grains on the ZrO2 matrix, in two distinct morphologies: equiaxial grains and platelets. The composites (Ce,Y)-TZP/Al2O3 presented average values of elastic moduli, Vickers hardness and fracture toughness of 228.3 ± 6.5 GPa, 1427 ± 46 HV e 11.3 ± 0.4 MPa m1/2, respectively. An inversely proportional relationship is observed between the roughness and the bending strength, since the 3Y-TZP samples presented a average strength of 860.7 ± 81 MPa (as-sintered) and 965.4 ± 93 MPa (polished) while the (Ce,Y)-TZP/Al2O3 composites presented average strength of 810.6 ± 147 MPa (as-sintered) and 952.6 ± 88 MPa (polished). CONCLUSIONS: The composites (Ce,Y)-TZP/Al2O3 showed high resistance to degradation in saliva and adequate properties for use as dental implants. Values of flexural strength (>950 MPa) and Weibull modulus (m > 10) were similar to the conventional 3Y-TZP ceramics. Moreover, its hardness, elastic modulus and fracture toughness were higher than those obtained for 3Y-TZP. The expressive values of KIC obtained for (Ce,Y)-TZP/Al2O3 composites are results of association of different toughening mechanisms acting simultaneously in the material.

Effect of hydrothermal aging on the properties of zirconia with different levels of translucency.

OBJECTIVES: The aim of this study was to evaluate the effect of hydrothermal aging on the mechanical properties and translucency of dental zirconia with different levels of translucency. METHODS: Three different types of dental yttria-stabilized zirconia were used: 3Y-TZP (ZrO2 - 3 mol.% Y2O3) of medium opacity (designated Z3OP), 3Y-TZP of medium translucency (Z3MT), and 5Y-PSZ (ZrO2 - 5 mol.% Y2O3) of high translucency (Z5HT). A total of 120 specimens were sintered (n = 40 specimens/group). The control group (sintered→polished→heat-treated) and the aged group (sintered→polished→heat-treated→hydrothermally degraded at 134 °C, 2 bar, 5h) were characterized by relative density, quantitative phase analysis by X-ray diffraction using the Rietveld method, microstructural analysis by scanning electron microscopy, surface roughness and translucency. All groups were submitted to a biaxial flexural strength test. Data analysis using Kruskal-Wallis, Nemenyi (p-value = 0.05), and Weibull statistics were used. RESULTS: All sintered specimens presented full densification. After aging, an increase of the m-ZrO2 phase content was observed for the Z3OP group. On the other hand, Z3MT and Z5HT did not show any m-ZrO2 phase, indicating resistance to the hydrothermal degradation. Smaller grains were observed in the Z3MT group in relation to Z3OP group and the Z5HT group presented a bimodal grain distribution, where the largest grains were associated to cubic ZrO2. Z3OP exhibited a slight increase in roughness as a function of degradation, while the roughness remained statistically stable in the other groups. Translucency was little influenced by degradation, but considerably affected by increasing thickness. The Z5HT samples were the group with the highest translucency among the control groups. Z3OP exhibited the highest flexural strength, while being the most susceptible to hydrothermal degradation. The lowest values were presented by Z5HT in all groups, due to the high concentration of c-ZrO2 grains. CONCLUSION: Hydrothermal aging is less critical to the flexural strength of zirconia-based materials than the materials' composition and microstructure. Z5HT zirconia showed the highest translucency, however the measured difference is not visually perceptible. Z5HT was considered the most resistant to hydrothermal degradation.